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HRID 81622作成日:2026年10月26日

Cesium carbonate → 2,3-Dichloro-5-(2,2-diethoxyethoxy)pyridine

https://huagongshe.com/reaction/81622

反応式

関与物質

役割名称HCID仕込み量
反応物Cesium carbonateHCID 10796—
反応物DimethylacetamideHCID 31374—
反応物Ethane, 2-bromo-1,1-diethoxy-HCID 74852—
反応物2,3-Dichloro-5-hydroxypyridineHCID 14391672—
溶媒Ethyl AcetateHCID 8857—
生成物2,3-Dichloro-5-(2,2-diethoxyethoxy)pyridineHCID 8664589688.4%

反応条件

温度100 °C

反応手順

Bromoacetaldehyde diethyl acetal (2.74 ml, 18.3 mmol) and cesium carbonate (9.93 g, 30.5 mmol) were added to an N,N-dimethylacetamide solution (10 ml) of 5,6-dichloropyridin-3-ol (1.0 g, 6.10 mmol), and stirred under a nitrogen atmosphere at 100° C. for 16 hours. Saline solution and ethyl acetate were added to the reaction solution, the organic layer was washed with water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (Biotage, hexane:ethyl acetate=11:1 to 9:1) to obtain 2,3-dichloro-5-(2,2-diethoxyethoxy)pyridine (1.51 g, yield: 88%) as an orange oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08846700B2
出典データセットuspto-grants-2014_09
ORD IDord-499267f0d56448ea863eca0a72cb2f61
出典メモuspto-grants-2014_09